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है”ह”ह

IS 6213-3 (1971): Methods of Test for Pulp, Part III:Determination of Alpha, Beta and Gamma Cellulose in Pulp[CHD 15: Paper and its products]

IS : 6213 ( Part III)- 1971 ( Reaflinned 1992)

Indim Standard METHODS OF TEST FOR PULP

PART III DETERMINATIQN OF ALPHA, BETA AND GAMMA CELLULOSE JN PULP

( Second Reprint APRIL 1997 )

UDC 676.1 : 676.014.2 : [ 543.854.748 1

0 Copyriglrl 1971

BUREAU OF INDIAN STAND.4RDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

;r 2 November 1971

IS t 6213 (Port II1 ) - 1971 ( I~erNirwcd 1992 )

[It&m Stundard METHODS OF TEST FOR PULP

FAI”P 111 DETERMINATION OF ALPHA, BETA AND GAMMA CELLULOSE IN PULP

&$w Sectional Committee, CDC 15

SuRl N. ~ARASIIWAN

C-40 South Extension, R’ew Delhi 49

Members Represerding

SHRI N. J. &WWWI AlI India Fcdcration of blaster Printers, New Delhi Pkl#i R, f’%Y#4TRPWARAN ( Allem~~)

&RI \‘,J. RAKRIU Central Board of Excise & Customs SAW N. K. CHOWDRURI ( Altt-rtralc )

SHRI S. l3. BATRA Statiot\qry 8r Office Equipment Association of India, Calcutta

&q&r s. K:Uom National Test House, Calcutta Ssvl S. F. ~&-~LICK ( Altrmale )

SE&I A. P. CITAXRAV~W~I klinCtry of Defence ( R & D ) &~III A. C, DAS GUPT~ Chief Controller of Printing and Stationery, New

Delhi .

Ministry of Defence (TIC! )

Regicqal Research Laboratory ( CSIR ), Bhubaneswar Handmade Paper Institute, Pooua

Forest Research Institute & Colleges, Dehra Dun Srce Sararwaty Press Limited, Calcutta Iit$?~atiol! yf Paper Traders’ Association, Bombay Sasr DI~YI:YI)R~ Km411Jm

Sirnr Afivrbjp Clr~ar~bnt SHAH ( memo I fiaw D. P. .~.~TKbl\ Regional Research Laboratory ( CSIR ), Hyderabad

&ERI M. s. kkJidARASWA?dY (Ah&) SEBI M. A. JHANGIANI Dire;o,ra@ Qsneral of Supplies and Disposals, New

e SHBX h$ H. SAtVt4R ( Alkrrpatr )

$WRI s: K, w3ss4v4 India Tobacco Company Ltd, Calcutta !ittai~ Q? 8: W&W ( Ahwle 1

PRYt 6% kNA= Indian Paper Milla Aaociation, Calcutta SARI K. S. BHAR~AVA ( Alternate )

SHRI D. P. NATHANI Calcutta Paper Traders Association, Calcutta SHRI D. K. KOTH~RI ( Allnua& )

( Gnlinucd On pug0 2 )

BUREAU OF INDIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

IS: 6213 ( Part III ) - 1971

( Coariaurd ffonl pap 1 )

Strnr X. B. Ponnns All India Small PaperMills Association, Bombay SIIIU RAXWII Dn-rr The hILleta Hox Co of India,Ltd, Calcutta Dn N. V. C. Rno Direcc;rte General of Technical Development, New

SHRI A. N. Rao ( Allcrnafr ) Da D. C. TAPADAB Srrnr hf. s. ‘lkaor SIIIU D. D.\R Gwr~,

Director ( Chcm )

Institute of Paper Technology, Saharanpur Indian Paper Makers’ Associntion,~Calcutta Director General, ISI ( En-o&o Mm&r)

SHRI SATIEH CEANDER

Assistant Director ( Chem ), ISI

Methods of Test Subcommittee, CDC 15 : 2

Conven ff

DR D. C. TAPADAR

MnnbSU

Institute of Paper Technology, Sabuanpur

&m N. K. NAITRANI ( Altana)r to Dr D. C. Tapadar )

Snrtr V. J. BAXBE Central Board of Excise & Customs Ssisr N. K. CHOWDHTJBI ( Ahnrzlr )

Saax K. S. BHARUVA Rohtas Industries Limited, Dalmianagar Snar 0. L. DU~OAL The Ballarpur Paper & Strawboard Mills Ltd ( Shree

SHRI V. D. GVPTA ( Ahemlr) Gopal Division ), New Delhi

SHRI N. S. JABPAL ~oe~t~ti~ CK”

r Mills Ltd, Sangumagar Snnr MAN MOHAN SINQH

SHR~ G. M. MATHVB ( Al~rrurk) Institute & Colleges, Debra Dun

Da V. S. K. NAIB Orient Paper Mills Ltd. Calcutta Szis~ N. K. MOHATTA ( Alrmaf# )

2

IS:6213 (PBrtrn)- 1371

Indian Standard METHODS OF TEST FOR PULP

IART 111 DETERMINATION OF ALPHA, BETA AND GAMFlA CELLULOSE IN PULP

8. FOREWORD

0.1 This India Standard (Part III) was adopted by the Indian Stand- arda Institution on 26 June 1971, after the draft finalized by the Paper Sectional Committee had been approved by the Chemical Division Council.

0.2 For obtaining good quality of paper, it ia essential that the pul which goes into the manufacture of paper is roperly cooked and bleache mulation of this standard had been ta P

g . For- en up in order to guide the people

working in pulp and paper mills for the methods to be adopted for pulp ~analysis.

0.S In reportin f

the resulta of a test or analysis made in accordance with this standard, i the 6nal value, observed or calculated, C to be rounded off, it ahall be done in accordance with IS : 2-19608.

1. SCOPE

I.1 Thb standard (Part 111) prescribes the method of test for determina. tion of alpha, beta and gamma cellulose in pulp.

2. QUALITY OF REAGENTS

21 Unless otherwise specified, pure chemicals and distilled water (JR~ IS: lO70496Ot) freshly boiled and cooled, ahall be employed in the teab.

NOTE -I Pure chemicals ’ ahall mean chemiclrlr that do not contain impuritj~ which affect the results of analysis.

3. GENERAL

3.1 Plant cellulose ia not homogeneau in chemical composition. The residual high molecular weight fraction which is left behind when a mix- ture of pulp and 8.3 percent sodium hydroxide solution is filtered after the

*Rulea for -rounding off numerical values tSpecilicotioa for water, distilled quality t

r&d ). r&d).

3

1816213 (Part III)-1971

fibres have been initially swollen in a 17-5 percent sodium hydroxide solution under specified conditions, has been defined as alpha cellulose. The filtrate contains the short chain material and consists of beta and gamma ceiluioses. The fraction of cellulose which is capable of being reprecipitated by means of acid from the above solution is known as beta cellulose. The percentage of gamma cellulose may be obtained by subs &acting the sum of alpha and beta ceiiuioses from 100.

4. DETERMINATION OF ALPHA CELLULOSE

41 Re8geats

4.1.1 Sodium Hydroxide - 17.5 h O-1 percent by weight.

4.1.2 Sodium Hydroxide - 8.3 percent by weight.

4.2 Procedure

43.1 Take a representative sample of the pulp and shred it by hand ( not grind ). Keep one portion for determination of dry content. From the other portion weigh accurately a sample equivalent to approximately 3-O g of the moisture-free pulp. Transfer the same to a 250-ml beaker kept in a water-bath maintained at 20-O & 0*2”C. Take 75 ml of 17-5 ercent sodium hydroxide solution in a graduated cylinder and keep at 0°C in f the water-bath. Wet the pulp sample with 15 ml of this solutmn and dis- integrate it for one minute with the flat end of a glass rod; add 10 ml more of the sodium hydroxide solution to the pulp and mix for 45 seconds; and add 10 ml of sodium hydroxide solution and mix for 15 seconds, After the addition of 35 ml of caustic soda solution and disintegration, the pulp should be free from lumps, Stir and allow the mixture to stand in the water-bath for 3 more minutes. Add another 10 ml of sodium hydroxide solution and mix for 10 minutes more while adding the remaining 30 ml of caustic soda solution in three instalments of 10 ml a& at the intervals of 2.5, 5*0 and 7.5 minutes.

4.2.2 Leave the beaker with the contents in the waterrbath for another , 30 minutes. Now add 100 ml of distilled water at 20X, mix thoroughly with a glass rod and leave the diluted mixture in the watercbath for 30 minutes more. Filter the contents on w tared gooeh crucible by suction and collect the filtrate in a separate beaker. In case suspended Qbres are noticed in the filterate, pass it successively thro h the mat in the crucible till it is free from cellulose fibres. Rinse the bea er and residue with 25 ml Y of 8.3 percent sodium hydroxide solution at 20°C and transfer ail the fibres to the crucible. When applying suction, the pulp pad should be, kept covered with solution to prevent air being drawn through. Wash the residue with five 50-ml portions of distilled water at 20°C. Keep the filtrate aside for the determination of beta and gamma cellulose.

4

IS:6213 (-Part III)-1971

4.2.3 Place the crucible on another suction flask. Wash the residue in the crucible with 400 ml of distilled water at 20°C and subsequently with 40 ml of 10 percent acetic acid solution at 20°C. Allow a soaking period of 5 minutes before applying the suction. Wash the residue again with distilled water till it is free from acetic acid as indicated by litmus paper. Dry the crucible in an oven at 103 f 2°C and transfer the contents to a weighing bottle. Dry it to a constant weight.

4.3 Calculation-Carry out two determinations and calculate the per- centage of alpha cellulose as follows:

100 a x=--_ m

where 1 ’ x = alpha cellulose percentage by weight,

a = weight of precipitate in g, and

m = weight of pulpin g calculated on oven-dry basis.

Report the result as a mean of two determinations to two places of decimal. The results should check within 0.2 percent.

5. DETERMINATION OF~BETA CELLULOSE

5.1 Reagents

5.1.1 Acetic Acid

5.2 Procedure -Transfer the filtrate and washings from alpha cellulose determination to a 500-ml flask and make up the volume to the mark with distilled water. Shake well and pipette out 100 ml of the solution in a 250-ml beaker. Precipitate the beta cellulose by gradually adding acetic acid keeping the solution well stirred with a glass rod. Heat the mixture on a water-bath for 30 minutes to coagulate the precipitate. Filter and wash with hot distilled water till free from acid. Set aside the filtrate for

-gamma cellulose determination. Dry at 103 f 2°C in an air oven and weigh. Ignite the material so that allowance can be made for any ash.

5.3 Calculation -The weight of beta cellulose in 100 ml of solution being known, report it on the basis of 100 g of oven-dry pulp sample.

6. DETERMINATION OF GAMMA CELLULOSE

6.1 Reagents

6.1.1 Potassium Dichromate - 9 percent by weight.

6.1.2 Sulfihuric Acid - specific gravity 1.84.

5

IS : 6213 _( Part III ) - 1971

61.3 Ferrous Ammonium Sulfihate Solution-Make by dissolving 159.9 g of ferrous ammonium sulphate and add 5 ml of 10 percent sulphuric acid in one litre.

6.2 Procedure-Take 50 ml of the filtrateffom beta cellulose determina- tion and add 8 ml of 9 percent solution of potassium dichromate followed by 50 ml of sulphuric acid. Boil the mixture for exactly 3.5 minutes. Let it cool for 30 minutes. Titrate with ferrous ammonium sulphate solution using potassium ferricyanide as an external indicator.

1 g of KsCrsO, = 0.137 5 of gamma cellulose.

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